CN114950312A - Preparation device and method of industrial salicylic acid - Google Patents
Preparation device and method of industrial salicylic acid Download PDFInfo
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- CN114950312A CN114950312A CN202210486891.0A CN202210486891A CN114950312A CN 114950312 A CN114950312 A CN 114950312A CN 202210486891 A CN202210486891 A CN 202210486891A CN 114950312 A CN114950312 A CN 114950312A
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- sodium salicylate
- lifting cylinder
- lifting
- pipe
- wall
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- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 title claims abstract description 76
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229960004889 salicylic acid Drugs 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 title claims description 20
- ABBQHOQBGMUPJH-UHFFFAOYSA-M Sodium salicylate Chemical compound [Na+].OC1=CC=CC=C1C([O-])=O ABBQHOQBGMUPJH-UHFFFAOYSA-M 0.000 claims abstract description 89
- 229960004025 sodium salicylate Drugs 0.000 claims abstract description 89
- 238000003756 stirring Methods 0.000 claims abstract description 78
- 238000001035 drying Methods 0.000 claims abstract description 40
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims abstract description 10
- 235000017491 Bambusa tulda Nutrition 0.000 claims abstract description 10
- 241001330002 Bambuseae Species 0.000 claims abstract description 10
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims abstract description 10
- 239000011425 bamboo Substances 0.000 claims abstract description 10
- 230000001737 promoting effect Effects 0.000 claims abstract description 6
- 230000008676 import Effects 0.000 claims abstract 4
- 239000007788 liquid Substances 0.000 claims description 38
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 230000000087 stabilizing effect Effects 0.000 claims description 21
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 16
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 10
- 230000007246 mechanism Effects 0.000 claims description 10
- 238000005507 spraying Methods 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 9
- 238000001556 precipitation Methods 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000001569 carbon dioxide Substances 0.000 claims description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 8
- 238000003916 acid precipitation Methods 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 5
- 239000004299 sodium benzoate Substances 0.000 claims description 5
- 235000010234 sodium benzoate Nutrition 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 230000006835 compression Effects 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- BGOFCVIGEYGEOF-UJPOAAIJSA-N helicin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=CC=C1C=O BGOFCVIGEYGEOF-UJPOAAIJSA-N 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000011085 pressure filtration Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000001291 vacuum drying Methods 0.000 description 12
- 230000001133 acceleration Effects 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- NESLWCLHZZISNB-UHFFFAOYSA-M sodium phenolate Chemical compound [Na+].[O-]C1=CC=CC=C1 NESLWCLHZZISNB-UHFFFAOYSA-M 0.000 description 2
- 208000010444 Acidosis Diseases 0.000 description 1
- BSYNRYMUTXBXSQ-UHFFFAOYSA-N Aspirin Chemical compound CC(=O)OC1=CC=CC=C1C(O)=O BSYNRYMUTXBXSQ-UHFFFAOYSA-N 0.000 description 1
- 235000001553 Betula platyphylla Nutrition 0.000 description 1
- 241001313086 Betula platyphylla Species 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 208000010201 Exanthema Diseases 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 208000008454 Hyperhidrosis Diseases 0.000 description 1
- 241000124033 Salix Species 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 229960001138 acetylsalicylic acid Drugs 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000007950 acidosis Effects 0.000 description 1
- 208000026545 acidosis disease Diseases 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 210000004087 cornea Anatomy 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005489 elastic deformation Effects 0.000 description 1
- 201000005884 exanthem Diseases 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 230000036387 respiratory rate Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000035900 sweating Effects 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 230000008673 vomiting Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/16—Evaporating by spraying
- B01D1/18—Evaporating by spraying to obtain dry solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/003—Filters in combination with devices for the removal of liquids
- B01D36/008—Means to filter or treat the separated liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/007—Feed or outlet devices as such, e.g. feeding tubes provided with moving parts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/02—Preparation of carboxylic acids or their salts, halides or anhydrides from salts of carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/15—Preparation of carboxylic acids or their salts, halides or anhydrides by reaction of organic compounds with carbon dioxide, e.g. Kolbe-Schmitt synthesis
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/005—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the outlet side being of particular interest
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/007—Aspects relating to the heat-exchange of the feed or outlet devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/0009—Coils
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00162—Controlling or regulating processes controlling the pressure
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- Chemical & Material Sciences (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of salicylic acid preparation, and discloses a preparation device of industrial salicylic acid, which comprises a sodium salicylate generation tank body, a feeding pipe, a vent pipe, a drying pipe and a discharge pipe, wherein the feeding pipe, the vent pipe and the drying pipe are communicated with the top of the sodium salicylate generation tank body; the stirring rod comprises a first rod body and a lifting cylinder connected to the bottom of the first rod body, the first rod body is rotatably connected to the top of the sodium salicylate generating tank body, a plurality of stirring blades are arranged on the outer wall of the lifting cylinder, and the inner cavity of the lifting cylinder is hollow; the spiral promotes the body, and the vertical fixed connection of spiral promotes the body is on the inner wall of a promotion section of thick bamboo, and the promotion import has been seted up to the bottom of a promotion section of thick bamboo, and the promotion export has been seted up at the top, and the bottom that the spiral promoted the body is less than promoting the import, and the top is higher than promoting the export. The invention can improve the production efficiency.
Description
Technical Field
The invention relates to the technical field of salicylic acid preparation, in particular to a device and a method for preparing industrial salicylic acid.
Background
Salicylic acid is a fat-soluble organic acid with the chemical formula C 7 H 6 O 3 . The appearance is white crystalline powder, and the melting point is 158-161 ℃. It is an important fine chemical raw material in willow bark, folium Callicarpae Formosanae and Betula platyphylla in nature, and can be used for preparing medicine such as aspirin.
Salicylic acid is stable at normal temperature and rapidly decomposed into phenol and carbon dioxide by heating. Has the general property of partial acid. It can irritate skin and mucous membrane, and has corrosive effect due to its reaction with protein in body tissue. Can make cornea stripped after proliferation. It is less toxic than phenol, but can cause vomiting, diarrhea, headache, sweating, rash, increased respiratory rate, acidosis and excitement when taken in large amounts.
At present, various salicylic acid production methods exist, and it is common that phenol and sodium hydroxide are firstly reacted to produce sodium phenolate; then drying in a vacuum drying mode to obtain powdery sodium phenolate; then introducing carbon dioxide under the condition of several atmospheric pressures to carry out hydroxylation reaction, adding distilled water after the reaction is finished, heating, stirring and dissolving, then concentrating to obtain sodium salicylate solution, decoloring and filter-pressing the solution, then sending the solution into a precipitation tank, carrying out acid precipitation by using sulfuric acid, and finally separating by using a centrifugal machine to obtain the salicylic acid.
Disclosure of Invention
In view of this, the present invention provides an apparatus and a method for preparing industrial salicylic acid, so as to achieve the effect of improving the production efficiency.
In order to achieve the purpose, the invention provides a preparation device and a preparation method of industrial salicylic acid, which adopt the following technical scheme: a preparation device of industrial salicylic acid comprises,
the device comprises a sodium salicylate generating tank body, a feeding pipe, a vent pipe, a drying pipe and a discharge pipe, wherein the feeding pipe, the vent pipe and the drying pipe are communicated with the top of the sodium salicylate generating tank body;
the stirring rod is provided with a driving mechanism for driving the stirring rod to rotate, the stirring rod comprises a first rod body and a lifting cylinder connected to the bottom of the first rod body, the first rod body is rotatably connected to the top of the sodium salicylate generating tank body, the outer wall of the lifting cylinder is provided with a plurality of stirring blades, and the inner cavity of the lifting cylinder is hollow;
the spiral lifting body is vertically and fixedly connected to the inner wall of the lifting barrel, a lifting inlet is formed in the bottom of the lifting barrel, a lifting outlet is formed in the top of the lifting barrel, the bottom of the spiral lifting body is lower than the lifting inlet, and the top of the spiral lifting body is higher than the lifting outlet.
Further, the bottom of promoting a section of thick bamboo is vertical to be provided with the second body of rod, the second body of rod rotate connect in the bottom that the sodium salicylate generated the jar body.
Furthermore, the first rod body, the spiral lifting body and the second rod body are all hollow, the top of the spiral lifting body is communicated with the bottom of the first rod body, and the bottom of the spiral lifting body is communicated with the top of the second rod body;
actuating mechanism including set up in the support frame and the vertical setting in sodium salicylate generates jar body top in drive motor on the support frame, the last initiative tooth that is provided with of drive motor, be provided with on the outer wall of the first body of rod with the driven tooth that the initiative tooth engaged with, the support frame and drive motor all is located the lateral part of the first body of rod.
Further, be provided with the insulation cover on the outer wall that the sodium salicylate generated the jar body, be provided with spiral helicine auxiliary heating pipe on the outer wall that the sodium salicylate generated the jar body, the middle part of auxiliary heating pipe is located the insulation cover with between the outer wall that the sodium salicylate generated the jar body, both ends all are located the outside of insulation cover.
Furthermore, the end part of the second rod body is communicated with one end of the auxiliary heat pipe.
Furthermore, a plurality of flow guide shells are arranged on the outer wall of the lifting cylinder, the cross sections of the flow guide shells are fan-shaped, flow guide channels penetrate through the flow guide shells, one ends of the flow guide channels are communicated with the inner cavity of the sodium salicylate generation tank body, the other ends of the flow guide channels are communicated with the lifting inlet, and the lifting cylinder is in a first state or a second state during working;
when the lifting cylinder is in the first state, the lifting cylinder rotates along the X direction, the arc-shaped edge of the cross section of the diversion shell drives liquid to flow towards the direction far away from the lifting cylinder, and the spiral lifting body drives the liquid to move downwards;
when the lifting cylinder is in the second state, the lifting cylinder rotates along the-X direction, the guide channel guides liquid into the lifting cylinder, and the spiral lifting body drives the liquid to move upwards.
Further, stirring vane including connecting portion and vertical set up in connecting portion keep away from promote a stirring portion of one end, the cross section of stirring portion is arc or slope form, works as promote a section of thick bamboo when being in when the second state, stirring portion drive liquid orientation promote a direction flow of section of thick bamboo.
Furthermore, a rotating ring is horizontally and rotatably arranged on the inner wall of the sodium salicylate generating tank body, a plurality of vertical auxiliary sheets are arranged on the inner wall of the rotating ring, the auxiliary sheets are lower than the lifting outlet, an annular one-way ring is arranged between the free ends of all the auxiliary sheets, and a plurality of one-way bodies are hinged to the inner wall of the one-way ring;
the one-way ring is provided with a plurality of connecting seats, an elastic piece which is continuously in a compression state is arranged between each connecting seat and the one-way body, the inner wall of the one-way ring is also provided with a plurality of supporting blocks, and one side of each one-way body, which is far away from the elastic piece, is provided with one supporting block;
a plurality of L-shaped stabilizing pieces are arranged on the inner wall of the sodium salicylate generating tank body, a stabilizing ring is horizontally arranged between the free ends of all the stabilizing pieces, the top of the stabilizing ring movably abuts against the bottom of the supporting block, and the inner wall of the stabilizing ring movably abuts against the outer wall of the lifting cylinder;
the outer wall of the lifting cylinder is provided with a plurality of unidirectional teeth, and the cross sections of the unidirectional teeth are fan-shaped;
when the lifting cylinder is in the first state, the arc-shaped edge of the cross section of the one-way tooth acts on the one-way body and drives the elastic piece to further compress;
when the lifting cylinder is in the second state, the diameter edge of the cross section of the one-way tooth props against the free end of the one-way body, and the side part of the one-way body props against the supporting block.
Further, the device also comprises a decolorizing tank, a filter press, a settling tank and a centrifuge which are connected in sequence, wherein the decolorizing tank is communicated with the discharge pipe.
The present invention also provides a method for preparing salicylic acid using the apparatus for preparing industrial salicylic acid as described above, comprising the steps of,
s1, closing valves on the vent pipe, the drying pipe and the discharge pipe, and adding the phenol and the sodium hydroxide solution into the sodium salicylate generation tank body through the feed pipe;
s2, covering a sealing cover of the feeding pipe, and driving a stirring rod and a stirring blade to rotate by a driving mechanism until the reaction is finished;
s3, opening a valve on the drying pipe, starting a vacuum pump communicated with the drying pipe, heating the sodium salicylate generating tank body, rotating a stirring rod and a stirring blade, enabling liquid to enter the lifting cylinder from the lifting inlet, and spraying the liquid from the lifting outlet after being lifted by the spiral lifting body until powdery sodium benzoate is obtained;
s4, after the temperature in the sodium salicylate generating tank body is reduced, closing the vacuum pump and the valve on the drying pipe, opening the valve on the vent pipe, and conveying carbon dioxide into the sodium salicylate generating tank body through the conveying pump;
s5, after the vent pipe is closed, distilled water is fed into the sodium salicylate generating tank through the feeding pipe, and the temperature is raised and the mixture is stirred;
s6, opening a valve on the drying pipe, starting a vacuum pump communicated with the drying pipe, heating the sodium salicylate generating tank body, rotating a stirring rod and a stirring blade, enabling liquid to enter the lifting cylinder from the lifting inlet, and spraying the liquid from the lifting outlet after being lifted by the spiral lifting body to obtain a sodium salicylate solution;
s7, opening a valve on a discharge pipe, introducing the solution into a decoloring tank, and decoloring by using activated carbon;
s8, introducing the decolored solution into a pressure filter for pressure filtration, and then introducing the solution into a precipitation tank;
s9, adding sulfuric acid into the tank precipitation tank for acid precipitation;
and S10, centrifuging the material after acid precipitation to obtain the salicylic acid.
The preparation device of the industrial salicylic acid provided by the invention has the beneficial effects that: firstly, preparing a sodium salicylate solution, and then carrying out subsequent decolorization, filtration, precipitation, acidification, centrifugation and the like, wherein the core of the method is to distinguish the method and equipment for preparing the sodium salicylate solution from the prior art, and the subsequent processing method used after the sodium salicylate solution is produced is the same as the equipment and method on the market and is the prior art; it should also be understood that even if the subsequent manufacturing process is different, the method and/or the device of the present application can be used for manufacturing the product within the protection scope of the present application.
When the sodium salicylate solution is produced, firstly, valves (which are conventional valves, such as ball valves, butterfly valves and electromagnetic valves) on an air pipe, a drying pipe and a discharge pipe are closed, and phenol and sodium hydroxide solution are added into a sodium salicylate generation tank body through a feeding pipe; covering a sealing cover of the feeding pipe, and driving a stirring rod and a stirring blade to rotate by a driving mechanism until the reaction is finished;
then opening a valve on the drying pipe, starting a vacuum pump communicated with the drying pipe, heating the sodium salicylate generating tank body, rotating a stirring rod and a stirring blade, enabling liquid to enter a lifting cylinder from a lifting inlet, and spraying the liquid from a lifting outlet after being lifted by a spiral lifting body until powdery sodium benzoate is obtained; after the temperature in the sodium salicylate generating tank body is reduced, closing the vacuum pump and the valve on the drying pipe, opening the valve on the vent pipe, and conveying carbon dioxide into the sodium salicylate generating tank body through the conveying pump for reaction; after the reaction is finished, closing the vent pipe, feeding distilled water into the sodium salicylate generation tank through the feeding pipe, and heating and stirring;
and finally, opening a valve on the drying pipe, starting a vacuum pump communicated with the drying pipe, heating the sodium salicylate generating tank body, rotating the stirring rod and the stirring blade, enabling the liquid to enter the lifting cylinder from the lifting inlet, and spraying the liquid from the lifting outlet after being lifted by the spiral lifting body to obtain the sodium salicylate solution.
Wherein the liquid level of the solution is lower than the lifting outlet and higher than the lifting inlet in the whole reaction process; during the reaction between sodium hydroxide and phenol or other reactions or during vacuum drying, the stirring rod and the stirring blade can rotate, so that the reaction is accelerated; the stirring rod and the stirring blades can rotate in the X direction and the-X direction, so that when phenol reacts with sodium hydroxide and subsequent distilled water and the like are dissolved, the solution can be kept at a concentrated position as much as possible by rotating along the X direction, the reaction and the dissolution can be accelerated, and when the solution rotates along the-X direction, the solution enters the lifting cylinder from the lifting inlet, flows upwards under the lifting action of the spiral lifting body and is finally spilled outwards from the lifting outlet, so that the solutions at different positions can be mixed, and the reaction or the dissolution is accelerated;
moreover, when vacuum drying, whole in-process puddler is all to rotating along-X, just so can raise solution, later outwards spill from promoting the export, and unrestrained in-process, because the promotion section of thick bamboo at this moment also is in the rotation state continuously, so solution can be better dispersed and come, just so area of contact between increase solution that can be very big and the air, thereby very big acceleration the evaporation of water, vacuum drying's speed of being obtains very big improvement, and the production efficiency is improved.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment of an apparatus for preparing industrial salicylic acid according to the present invention;
FIG. 2 is an enlarged view of portion A of FIG. 1;
FIG. 3 is a sectional view of an embodiment of an apparatus for preparing industrial salicylic acid according to the present invention;
FIG. 4 is an enlarged view of portion B of FIG. 3;
FIG. 5 is an enlarged view of portion C of FIG. 3;
FIG. 6 is an enlarged view of portion D of FIG. 3;
FIG. 7 is a schematic view of an embodiment of a stirring rod part of the apparatus for preparing industrial salicylic acid according to the present invention;
fig. 8 is an enlarged view of portion E of fig. 7;
FIG. 9 is a sectional view of an embodiment of a stirring rod part of an apparatus for manufacturing industrial salicylic acid according to the present invention;
fig. 10 is an enlarged view of portion F of fig. 9;
FIG. 11 is a schematic view of an embodiment of a stirring blade and a spiral lifting body in the device for preparing industrial salicylic acid provided by the present invention.
Reference numbers in the figures: 1. a sodium salicylate generating tank body; 2. a feed tube; 3. a breather pipe; 4. a drying tube; 5. a discharge pipe; 6. a stirring rod; 6a, a first rod body; 6b, a lifting cylinder; 6c, a second rod body; 7. a stirring blade; 7a, a connecting part; 7b, a stirring part; 8. a lift inlet; 9. a lift outlet; 10. a spiral lifting body; 11. a support frame; 12. a drive motor; 13. a driving tooth; 14. a passive tooth; 15. a thermal insulation sleeve; 16. an auxiliary heat pipe; 17. a guide shell; 18. a flow guide channel; 19. a rotating ring; 20. an auxiliary sheet; 21. a unidirectional ring; 22. a unidirectional body; 23. a connecting seat; 24. an elastic member; 25. a support block; 26. a stabilizer; 27. a stabilizing ring; 28. a unidirectional tooth.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the drawings of the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention, are within the scope of the invention.
As shown in figures 1 to 11 of the drawings,
a device for preparing industrial salicylic acid, comprising:
the device comprises a sodium salicylate generating tank body 1, a feeding pipe 2, a vent pipe 3, a drying pipe 4 and a discharge pipe 5, wherein the feeding pipe 2 is communicated with the top of the sodium salicylate generating tank body 1;
the stirring rod 6 is arranged on the sodium salicylate generating tank body 1 and is used for driving the stirring rod 6 to rotate, the stirring rod 6 comprises a first rod body 6a and a lifting cylinder 6b connected to the bottom of the first rod body 6a, the first rod body 6a is rotatably connected to the top of the sodium salicylate generating tank body 1, a plurality of stirring blades 7 are arranged on the outer wall of the lifting cylinder 6b, and the inner cavity of the lifting cylinder 6b is hollow;
the spiral lifting body 10 is vertically and fixedly connected to the inner wall of the lifting barrel 6b, a lifting inlet 8 is formed in the bottom of the lifting barrel 6b, a lifting outlet 9 is formed in the top of the lifting barrel 6b, the bottom of the spiral lifting body 10 is lower than the lifting inlet 8, and the top of the spiral lifting body is higher than the lifting outlet 9.
The bottom of the lifting cylinder 6b is vertically provided with a second rod body 6c, and the second rod body 6c is rotatably connected to the bottom of the sodium salicylate generating tank body 1.
The first rod body 6a, the spiral lifting body 10 and the second rod body 6c are all hollow, the top of the spiral lifting body 10 is communicated with the bottom of the first rod body 6a, and the bottom of the spiral lifting body is communicated with the top of the second rod body 6 c;
actuating mechanism including set up in the sodium salicylate generates support frame 11 and vertical set up in 1 top of the jar body drive motor 12 on the support frame 11, be provided with driving tooth 13 on the drive motor 12, be provided with on the outer wall of the first body of rod 6a with driven tooth 14 that driving tooth 13 meshed mutually, the support frame 11 and drive motor 12 all is located the lateral part of the first body of rod 6 a.
Be provided with the insulation cover 15 on the outer wall of the sodium salicylate generation jar body 1, be provided with spiral helicine auxiliary heating pipe 16 on the outer wall of the sodium salicylate generation jar body 1, auxiliary heating pipe 16's middle part is located insulation cover 15 with between the outer wall of the sodium salicylate generation jar body 1, both ends all are located insulation cover 15's outside. The end of the second rod 6c is communicated with one end of the auxiliary heat pipe 16.
The outer wall of the lifting cylinder 6b is provided with a plurality of guide shells 17, the cross sections of the guide shells 17 are fan-shaped, guide channels 18 are formed by penetrating through the guide shells 17, one ends of the guide channels 18 are communicated with the inner cavity of the sodium salicylate generating tank body 1, the other ends of the guide channels 18 are communicated with the lifting inlet 8, and the lifting cylinder 6b is in a first state or a second state during working;
when the lifting cylinder 6b is in the first state, the lifting cylinder 6b rotates along the X direction, the arc-shaped edge of the cross section of the diversion shell 17 drives the liquid to flow towards the direction far away from the lifting cylinder 6b, and the spiral lifting body 10 drives the liquid downwards;
when the lifting cylinder 6b is in the second state, the lifting cylinder 6b rotates in the-X direction, the guide passage 18 guides the liquid into the lifting cylinder 6b, and the spiral lifting body 10 drives the liquid upward.
The stirring blade 7 comprises a connecting part 7a and a stirring part 7b vertically arranged at one end of the connecting part 7a far away from the lifting cylinder 6b, the cross section of the stirring part 7b is arc-shaped or inclined, and when the lifting cylinder 6b is in the second state, the stirring part 7b drives liquid to flow towards the lifting cylinder 6 b.
A rotating ring 19 is horizontally and rotatably arranged on the inner wall of the sodium salicylate generating tank body 1, a plurality of vertical auxiliary pieces 20 are arranged on the inner wall of the rotating ring 19, the auxiliary pieces 20 are lower than the lifting outlet 9, an annular one-way ring 21 is arranged between the free ends of all the auxiliary pieces 20, and a plurality of one-way bodies 22 (in a U shape, the upper end and the lower end of each one-way body are respectively hinged with the upper side and the lower side of the one-way ring 21) are hinged on the inner wall of the one-way ring 21;
the one-way ring 21 is provided with a plurality of connecting seats 23, an elastic part 24 which is continuously in a compression state is arranged between each connecting seat 23 and the one-way body 22, the inner wall of the one-way ring 21 is also provided with a plurality of supporting blocks 25, and one side of each one-way body 22, which is far away from the elastic part 24, is provided with one supporting block 25;
a plurality of L-shaped stabilizing members 26 are arranged on the inner wall of the sodium salicylate generating tank body 1, a stabilizing ring 27 is horizontally arranged between the free ends of all the stabilizing members 26, the top of the stabilizing ring 27 movably abuts against the bottom of the supporting block 25, and the inner wall of the stabilizing ring 27 movably abuts against the outer wall of the lifting cylinder 6 b;
the outer wall of the lifting cylinder 6b is provided with a plurality of one-way teeth 28, and the cross section of each one-way tooth 28 is in a sector shape;
when the lifting cylinder 6b is in the first state, the arc-shaped edge of the cross section of the one-way tooth 28 acts on the one-way body 22 and drives the elastic piece 24 to further compress;
when the lifting cylinder 6b is in the second state, the diameter side of the cross section of the one-way tooth 28 abuts against the free end of the one-way body 22, and the side of the one-way body 22 abuts against the supporting block 25.
The device also comprises a decolorizing tank, a filter press, a settling tank and a centrifuge which are connected in sequence, wherein the decolorizing tank is communicated with the discharge pipe 5.
The present invention also provides a method for preparing salicylic acid using the apparatus for preparing industrial salicylic acid as described above, comprising the steps of,
s1, closing valves on the vent pipe 3, the drying pipe 4 and the discharge pipe 5, and adding phenol and sodium hydroxide solution into the sodium salicylate generation tank body 1 through the feeding pipe 2;
s2, covering the sealing cover of the feeding pipe 2, and driving the stirring rod 6 and the stirring blade 7 to rotate by the driving mechanism until the reaction is finished;
s3, opening a valve on the drying pipe 4, starting a vacuum pump communicated with the drying pipe 4, heating the sodium salicylate generating tank body 1, rotating the stirring rod 6 and the stirring blade 7, enabling liquid to enter the lifting cylinder 6b from the lifting inlet 8, and spraying the liquid from the lifting outlet 9 after being lifted by the spiral lifting body 10 until powdery sodium benzoate is obtained;
s4, after the temperature in the sodium salicylate generating tank body 1 is reduced, closing the vacuum pump and the valve on the drying pipe 4, opening the valve on the vent pipe 3, and conveying carbon dioxide into the sodium salicylate generating tank body 1 through the conveying pump;
s5, after the vent pipe 3 is closed, distilled water is fed into the sodium salicylate generating tank body 1 through the feeding pipe 2, and the temperature is raised and the mixture is stirred;
s6, opening a valve on the drying pipe 4, starting a vacuum pump communicated with the drying pipe 4, heating the sodium salicylate generating tank body 1, rotating the stirring rod 6 and the stirring blade 7, enabling liquid to enter the lifting cylinder 6b from the lifting inlet 8, and spraying the liquid from the lifting outlet 9 after being lifted by the spiral lifting body 10 to obtain a sodium salicylate solution;
s7, opening a valve on the discharge pipe 5, introducing the solution into a decoloring tank, and decoloring by using activated carbon;
s8, introducing the decolored solution into a pressure filter for pressure filtration, and then introducing the solution into a precipitation tank;
s9, adding sulfuric acid into the tank precipitation tank for acid precipitation;
and S10, centrifuging the material after acid precipitation to obtain the salicylic acid.
Firstly, preparing a sodium salicylate solution, and then carrying out subsequent decolorization, filtration, precipitation, acidification, centrifugation and the like, wherein the core of the method is to distinguish the method and equipment for preparing the sodium salicylate solution from the prior art, and the subsequent processing method used after the sodium salicylate solution is produced is the same as the equipment and method on the market and is the prior art; it should also be understood that even if the subsequent manufacturing process is different, the method and/or apparatus of the present application can be used for manufacturing the product within the protection scope of the present application.
When the sodium salicylate solution is produced, firstly, valves (which are conventional valves, such as ball valves, butterfly valves and electromagnetic valves) on the vent pipe 3, the drying pipe 4 and the discharge pipe 5 are closed, and phenol and sodium hydroxide solution are added into a sodium salicylate generation tank body 1 through a feeding pipe 2; the sealing cover of the feeding pipe 2 is covered, and the driving mechanism drives the stirring rod 6 and the stirring blade 7 to rotate until the reaction is finished;
then opening a valve on the drying pipe 4, starting a vacuum pump communicated with the drying pipe 4, heating the sodium salicylate generating tank body 1, rotating the stirring rod 6 and the stirring blade 7, enabling the liquid to enter the lifting cylinder 6b from the lifting inlet 8, and spraying the liquid out from the lifting outlet 9 after being lifted by the spiral lifting body 10 until powdery sodium benzoate is obtained; after the temperature in the sodium salicylate generating tank body 1 is reduced, the vacuum pump and the valve on the drying pipe 4 are closed, the valve on the vent pipe 3 is opened, and carbon dioxide is conveyed into the sodium salicylate generating tank body 1 through the conveying pump for reaction; after the reaction is finished, closing the vent pipe 3, feeding distilled water into the sodium salicylate generating tank body 1 through the feeding pipe 2, and heating and stirring;
and finally, opening a valve on the drying pipe 4, starting a vacuum pump communicated with the drying pipe 4, heating the sodium salicylate generating tank body 1, rotating the stirring rod 6 and the stirring blade 7, enabling the liquid to enter the lifting cylinder 6b from the lifting inlet 8, and spraying the liquid from the lifting outlet 9 after being lifted by the spiral lifting body 10 to obtain a sodium salicylate solution.
Wherein the liquid level of the solution is lower than the lift outlet 9 and higher than the lift inlet 8 in the whole reaction process; in the reaction between sodium hydroxide and phenol or other reactions, or in the vacuum drying, the stirring rod 6 and the stirring blade 7 can rotate, so that the reaction is accelerated; in addition, the stirring rod 6 and the stirring blade 7 can rotate in the X direction and the-X direction, so that when phenol reacts with sodium hydroxide and subsequent distilled water and the like are dissolved, the solution can be kept at a concentrated position as much as possible by rotating along the X direction, the reaction and the dissolution can be accelerated, and when the solution rotates along the-X direction, the solution enters the lifting cylinder 6b from the lifting inlet 8, flows upwards under the lifting action of the spiral lifting body 10 and is finally spilled outwards from the lifting outlet 9, so that the solutions at different positions can be mixed, and the reaction or the dissolution can be accelerated;
moreover, when vacuum drying, whole in-process puddler 6 is all to rotating along-X, just so can raise solution, later spill from promoting export 9 to outside, and the in-process of spilling, because this moment the promotion section of thick bamboo 6b also continuously is in the rotating-state, so solution can be better be dispersed and come, just so can be very big increase solution and the area of contact between the air, thereby very big acceleration the evaporation of water, vacuum drying's speed of being obtain very big improvement, and the production efficiency is improved.
The second rod body 6c at the bottom of the lifting cylinder 6b and the first rod body 6a at the top of the sodium salicylate generation tank body 1 are in rotating and sealing connection with the sodium salicylate generation tank body 1, and even if carbon dioxide and solution with higher air pressure exist, the two rod bodies can be stably positioned in the sodium salicylate generation tank body 1; the second rod body 6c can firstly improve the position stability of the lifting cylinder 6b, and secondly, when in actual production and use, a pipeline for conveying a heating medium into the first rod body 6a is connected to the outside of the first rod body 6a, and the pipeline is in rotary sealing connection with the top of the first rod body 6 a; even if the first rod 6a rotates, the pipeline for conveying the heating medium can still be communicated with the first rod 6 a;
after entering the first rod 6a, the heating medium enters the spiral lifting body 10, the second rod 6c and the auxiliary heat pipe 16 in sequence; firstly because the heating medium is both located spiral lifting body 10 and second body of rod 6c, also is located auxiliary heat pipe 16 simultaneously, so can generate more comprehensive heating of the solution in the jar body 1 to sodium salicylate, heating effect and speed all be faster, simultaneously because the medium in auxiliary heat pipe 16 is from second body of rod 6c inflow, can also make the medium of same place used by a plurality of times like this to make thermal utilization ratio higher. Moreover, when carrying out vacuum drying, spiral lifting body 10 not only can promote the solution, can also all heat the solution at the in-process that promotes simultaneously for subsequent vacuum drying speed further obtains improving.
When phenol and sodium hydroxide react and subsequent distilled water is dissolved, if the solution needs to be better concentrated at the moment so as to accelerate the reaction, the stirring rod 6 and the stirring blade 7 rotate along the X direction at the moment, so that the solution entering the lifting cylinder 6b is little and cannot be lifted at the moment; at the moment, the outer wall of the diversion shell 17 and the stirring part 7b drive the liquid to move towards the direction far away from the lifting cylinder 6b, so that the solution entering the lifting cylinder 6b can be further reduced;
and when carrying out vacuum drying to and when mixing the solution of co-altitude not, puddler 6 orientation-X at this moment is to rotating, and the portion 7b that at first stirs can play a drive effect to the solution far away from lifting cylinder 6b for the better orientation of solution promotes a section of thick bamboo 6b and flows, and the opening of blower inlet 17 one end also can accelerate solution and enter into lifting cylinder 6b simultaneously, then is spilt after being rised by spiral lifting body 10, the whole drying rate of acceleration, and the mixing velocity and the degree of consistency of co-altitude solution not.
Moreover, when the stirring rod 6 rotates in the direction X, the one-way teeth 28 cannot drive the one-way ring 21 to rotate or hardly drive the one-way ring 21 to rotate, and the requirement on the rotational power of the lifting cylinder 6b is low, so that the abrasion to each structure is small; then, when the vacuum drying and the mixing of the solutions with different heights are carried out, the one-way teeth 28 are abutted against the one-way body 22, the one-way ring 21 is driven to rotate through the one-way body 22, and then the one-way ring 21 can drive all the auxiliary pieces 20 and the rotating ring 19 to rotate; because the auxiliary sheet 20 is positioned below the lifting outlet 9, when the solution is sprayed out of the lifting outlet 9, the wind generated by the auxiliary sheet 20 can also fan upwards; thus, if the auxiliary sheet 20 is used for vacuum drying, the drying speed can be further accelerated, and when the solutions with different heights are mixed, the auxiliary sheet 20 can play a beating role on the solutions, so that the solutions are dispersed into smaller droplets, and the dissolving or reacting speed can be faster.
When the lifting cylinder 6b rotates towards the direction X, the one-way teeth 28 drive the one-way body 22 to rotate, meanwhile, the elastic member 24 (i.e., the spring) is elastically deformed further, and after the elastic deformation, the one-way teeth 28 can pass over the one-way body 22, so that the one-way ring 21 cannot be driven to rotate; however, when the first rod 6a rotates along the direction-X, the one-way tooth 28 abuts against the free end of the one-way body 22, and the back of the one-way body 22 abuts against the supporting block 25, so that the one-way body 22 cannot rotate further, and at the same time, the one-way ring 21 is driven to rotate; and because the supporting block 25 exists, can prevent the elastic component 24 from taking place the damage better, guaranteed its life.
The stabilizing members 26 and the stabilizing rings 27 on the inner wall of the sodium salicylate generating tank body 1 can support the one-way rings 21, improve and protect the position stability and the shape stability of the one-way rings 21, and meanwhile, because the inner wall of the stabilizing rings 27 is movably attached to the outer wall of the lifting cylinder 6b, the position stability and the shape stability of the lifting cylinder 6b can be improved at the same time. And the stabilizing member 26 is positioned below the auxiliary plate 20, so that when the solution is sprayed from the lift outlet 9, the stabilizing member 26 can further disperse and retain the solution, thereby performing a certain acceleration.
In the present invention, unless otherwise explicitly specified or limited, for example, it may be fixedly attached, detachably attached, or integrated; can be mechanically or electrically connected; the terms may be directly connected or indirectly connected through an intermediate, and may be communication between two elements or interaction relationship between two elements, unless otherwise specifically limited, and the specific meaning of the terms in the present invention will be understood by those skilled in the art according to specific situations.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A preparation facilities of industry salicylic acid which characterized in that: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
the device comprises a sodium salicylate generating tank body (1), a feeding pipe (2) communicated with the top of the sodium salicylate generating tank body (1), a vent pipe (3), a drying pipe (4) and a discharge pipe (5) communicated with the bottom of the sodium salicylate generating tank body (1);
the stirring rod (6), a driving mechanism for driving the stirring rod (6) to rotate is arranged on the sodium salicylate generation tank body (1), the stirring rod (6) comprises a first rod body (6a) and a lifting cylinder (6b) connected to the bottom of the first rod body (6a), the first rod body (6a) is rotatably connected to the top of the sodium salicylate generation tank body (1), a plurality of stirring blades (7) are arranged on the outer wall of the lifting cylinder (6b), and the inner cavity of the lifting cylinder (6b) is hollow;
the spiral lifting body (10), the vertical fixed connection of spiral lifting body (10) in promote on the inner wall of a section of thick bamboo (6b), promote import (8) have been seted up to the bottom of promoting a section of thick bamboo (6b), promote export (9) have been seted up at the top, the bottom of spiral lifting body (10) is less than promote import (8), the top is higher than promote export (9).
2. The apparatus for preparing industrial salicylic acid according to claim 1, wherein: the bottom of lifting cylinder (6b) is vertically provided with a second rod body (6c), and second rod body (6c) is rotationally connected with the bottom of sodium salicylate generation tank body (1).
3. The apparatus for preparing industrial salicylic acid according to claim 2, wherein: the first rod body (6a), the spiral lifting body (10) and the second rod body (6c) are all hollow, the top of the spiral lifting body (10) is communicated with the bottom of the first rod body (6a), and the bottom of the spiral lifting body is communicated with the top of the second rod body (6 c);
actuating mechanism including set up in support frame (11) and the vertical setting in the sodium salicylate generates jar body (1) top drive motor (12) on support frame (11), be provided with driving tooth (13) on drive motor (12), be provided with on the outer wall of the first body of rod (6a) with driven tooth (14) that driving tooth (13) engaged with, support frame (11) and drive motor (12) all are located the lateral part of the first body of rod (6 a).
4. The apparatus for preparing industrial salicylic acid according to claim 3, wherein: be provided with insulation support (15) on the outer wall of the sodium salicylate generation jar body (1), be provided with spiral helicine auxiliary heating pipe (16) on the outer wall of the sodium salicylate generation jar body (1), the middle part of auxiliary heating pipe (16) is located insulation support (15) with between the outer wall of the sodium salicylate generation jar body (1), both ends all are located the outside of insulation support (15).
5. The apparatus for preparing industrial salicylic acid according to claim 4, wherein: the end part of the second rod body (6c) is communicated with one end of the auxiliary heat pipe (16).
6. The apparatus for preparing industrial salicylic acid according to claim 1, wherein: the outer wall of the lifting cylinder (6b) is provided with a plurality of flow guide shells (17), the cross sections of the flow guide shells (17) are fan-shaped, flow guide channels (18) penetrate through the flow guide shells (17), one ends of the flow guide channels (18) are communicated with the inner cavity of the sodium salicylate generating tank body (1), the other ends of the flow guide channels are communicated with the lifting inlet (8), and the lifting cylinder (6b) is in a first state or a second state during working;
when the lifting cylinder (6b) is in the first state, the lifting cylinder (6b) rotates along the X direction, the arc-shaped edge of the cross section of the diversion shell (17) drives liquid to flow in a direction away from the lifting cylinder (6b), and the spiral lifting body (10) drives the liquid to move downwards;
when the lifting cylinder (6b) is in the second state, the lifting cylinder (6b) rotates along the-X direction, the flow guide channel (18) guides liquid into the lifting cylinder (6b), and the spiral lifting body (10) drives the liquid upwards.
7. The apparatus for preparing industrial salicylic acid according to claim 6, wherein: stirring vane (7) including connecting portion (7a) and vertically set up in connecting portion (7a) are kept away from stirring portion (7b) of lifting cylinder (6b) one end, the cross-section of stirring portion (7b) is circular arc or slope form, works as lifting cylinder (6b) is in when the second state, stirring portion (7b) drive liquid orientation the direction of lifting cylinder (6b) flows.
8. The apparatus for preparing industrial salicylic acid according to claim 6, wherein: a rotating ring (19) is horizontally and rotatably arranged on the inner wall of the sodium salicylate generating tank body (1), a plurality of vertical auxiliary sheets (20) are arranged on the inner wall of the rotating ring (19), the auxiliary sheets (20) are lower than the lifting outlet (9), an annular one-way ring (21) is arranged between the free ends of all the auxiliary sheets (20), and a plurality of one-way bodies (22) are hinged on the inner wall of the one-way ring (21);
the one-way ring (21) is provided with a plurality of connecting seats (23), an elastic piece (24) which is continuously in a compression state is arranged between each connecting seat (23) and the one-way body (22), the inner wall of the one-way ring (21) is also provided with a plurality of supporting blocks (25), and one side of each one-way body (22) departing from the elastic piece (24) is provided with one supporting block (25);
a plurality of L-shaped stabilizing pieces (26) are arranged on the inner wall of the sodium salicylate generating tank body (1), a stabilizing ring (27) is horizontally arranged between the free ends of all the stabilizing pieces (26), the top of the stabilizing ring (27) movably abuts against the bottom of the supporting block (25), and the inner wall of the stabilizing ring (27) movably abuts against the outer wall of the lifting cylinder (6 b);
the outer wall of the lifting cylinder (6b) is provided with a plurality of one-way teeth (28), and the cross sections of the one-way teeth (28) are in a fan shape;
when the lifting cylinder (6b) is in the first state, the arc-shaped side of the cross section of the one-way tooth (28) acts on the one-way body (22) and drives the elastic piece (24) to further compress;
when the lifting cylinder (6b) is in the second state, the diameter edge of the cross section of the one-way tooth (28) is abutted against the free end of the one-way body (22), and the side part of the one-way body (22) is abutted against the supporting block (25).
9. The apparatus for preparing industrial salicylic acid according to claim 1, wherein: the device also comprises a decolorizing tank, a filter press, a settling tank and a centrifuge which are connected in sequence, wherein the decolorizing tank is communicated with the discharge pipe (5).
10. A method for preparing salicylic acid using the apparatus for preparing industrial salicylic acid according to claim 9, wherein: comprises the following steps of (a) carrying out,
s1, closing valves on the vent pipe (3), the drying pipe (4) and the discharge pipe (5), and adding the phenol and the sodium hydroxide solution into the sodium salicylate generation tank body (1) through the feeding pipe (2);
s2, covering a sealing cover of the feeding pipe (2), and driving a stirring rod (6) and a stirring blade (7) to rotate by a driving mechanism until the reaction is finished;
s3, opening a valve on the drying pipe (4), starting a vacuum pump communicated with the drying pipe (4), heating the sodium salicylate generating tank body (1), rotating the stirring rod (6) and the stirring blade (7), enabling liquid to enter the lifting cylinder (6b) from the lifting inlet (8), and spraying the liquid from the lifting outlet (9) after being lifted by the spiral lifting body (10) until powdery sodium benzoate is obtained;
s4, after the temperature in the sodium salicylate generating tank body (1) is reduced, closing the vacuum pump and the valve on the drying pipe (4), opening the valve on the vent pipe (3), and conveying carbon dioxide into the sodium salicylate generating tank body (1) through the conveying pump;
s5, after the vent pipe (3) is closed, distilled water is fed into the sodium salicylate generating tank body (1) through the feeding pipe (2), and the mixture is heated and stirred;
s6, opening a valve on the drying pipe (4), starting a vacuum pump communicated with the drying pipe (4), heating the sodium salicylate generating tank body (1), rotating the stirring rod (6) and the stirring blade (7), enabling liquid to enter the lifting cylinder (6b) from the lifting inlet (8), and spraying the liquid from the lifting outlet (9) after being lifted by the spiral lifting body (10) to obtain a sodium salicylate solution;
s7, opening a valve on a discharge pipe (5), and introducing the solution into a decoloring tank for decoloring by using activated carbon;
s8, introducing the decolored solution into a pressure filter for pressure filtration, and then introducing the solution into a precipitation tank;
s9, adding sulfuric acid into the tank precipitation tank for acid precipitation;
and S10, centrifuging the material after acid precipitation to obtain the salicylic acid.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116920662A (en) * | 2023-09-16 | 2023-10-24 | 江苏金桥油脂科技有限公司 | Hardened oil decoloration cauldron |
| CN117085349A (en) * | 2023-10-19 | 2023-11-21 | 上海中腾环保科技有限公司 | Efficient flash evaporation system and flash evaporation method thereof |
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| CN117085349B (en) * | 2023-10-19 | 2024-01-26 | 上海中腾环保科技有限公司 | Efficient flash evaporation system and flash evaporation method thereof |
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